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目的研制适用于采集工作场所空气中环氧乙烷(EO)的浸渍活性炭管,并建立配套的气相色谱测定方法。方法基于EO能与氢溴酸发生开环反应生成2-溴乙醇的原理,研制浸渍活性炭管,采集空气中EO,用二甲基甲酰胺解吸反应生成的2-溴乙醇后,经毛细管色谱柱分离,氢火焰离子化检测器检测。结果 EO在0.12~97.29 mg/L范围内线性关系良好,相关系数为0.99992;该方法的批内精密度相对标准偏差(RSD)为0.92%~3.53%,批间精密度RSD为2.80%~5.98%;平均衍生效率为99.70%~100.00%;平均解吸效率为85.00%~92.65%;定量下限为0.06 mg/L;最低定量质量浓度为0.02 mg/m3(以采集3.0 L空气计)。在室温下,样品可保存6 d;在4℃冰箱中,样品至少可保存8 d。结论研制的浸渍活性炭管及其配套的测定方法与现行国标方法比较,样品保存时间长、可长时间大量采样、操作方便、成本低,更适用于工作场所空气中EO的采样以及检测。
Objective To develop an impregnated activated carbon tube suitable for the collection of ethylene oxide (EO) in the air of the workplace and to establish a complete gas chromatographic method. Methods Based on the principle that EO can react with hydrobromic acid to produce 2-bromoethanol, an impregnated activated carbon tube was prepared. EO in air was collected and the 2-bromoethanol was desorbed by dimethylformamide. After the capillary column Separation, hydrogen flame ionization detector detection. Results The linearity of EO ranged from 0.12 to 97.29 mg / L, with a correlation coefficient of 0.99992. The relative standard deviation (RSD) was 0.92% ~ 3.53% and the inter-batch precision RSD was 2.80% ~ 5.98 The average derivatization efficiency was 99.70% -100.00%. The average desorption efficiency was 85.00% -92.65%. The lower limit of quantitation was 0.06 mg / L. The lowest concentration was 0.02 mg / m3. The sample can be stored for 6 days at room temperature and for at least 8 days in a 4 ° C freezer. Conclusion Compared with the current national standard method, the impregnated activated carbon tube and its measuring method developed in this paper have a long sample holding time, a large number of samples can be sampled for a long time, the operation is convenient and the cost is low. It is more suitable for the sampling and testing of EO in the air of the workplace.